US10843268B2 - Metal laminated and shaped object, aluminum-based powder for metal laminating and shaping, and method of manufacturing the same - Google Patents
Metal laminated and shaped object, aluminum-based powder for metal laminating and shaping, and method of manufacturing the same Download PDFInfo
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- US10843268B2 US10843268B2 US15/545,989 US201615545989A US10843268B2 US 10843268 B2 US10843268 B2 US 10843268B2 US 201615545989 A US201615545989 A US 201615545989A US 10843268 B2 US10843268 B2 US 10843268B2
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- 239000000843 powder Substances 0.000 title claims abstract description 132
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 54
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 53
- 239000002184 metal Substances 0.000 title claims abstract description 53
- 238000007493 shaping process Methods 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000010030 laminating Methods 0.000 title 1
- 239000002245 particle Substances 0.000 claims abstract description 64
- 239000001257 hydrogen Substances 0.000 claims abstract description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001301 oxygen Substances 0.000 claims abstract description 26
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 26
- 230000004927 fusion Effects 0.000 claims abstract description 6
- 238000009826 distribution Methods 0.000 claims abstract description 5
- 238000000790 scattering method Methods 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 43
- 239000000956 alloy Substances 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 42
- 239000011261 inert gas Substances 0.000 claims description 13
- 238000009690 centrifugal atomisation Methods 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 8
- 238000009689 gas atomisation Methods 0.000 claims description 5
- 230000007547 defect Effects 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 229910000861 Mg alloy Inorganic materials 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 11
- 239000012300 argon atmosphere Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 238000007872 degassing Methods 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910018566 Al—Si—Mg Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/141—Processes of additive manufacturing using only solid materials
- B29C64/153—Processes of additive manufacturing using only solid materials using layers of powder being selectively joined, e.g. by selective laser sintering or melting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
- B22F12/40—Radiation means
- B22F12/41—Radiation means characterised by the type, e.g. laser or electron beam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Definitions
- the present invention relates to metal lamination-shaping.
- patent literature 1 has disclosed a method of adding a sintering aid to an aluminum powder as needed, and sintering the aluminum powder by heating it in a nitrogen atmosphere containing water vapor at a predetermined partial pressure.
- Patent literature 1 describes that a sintered object having a high relative density is obtained by using a metal lamination-shaping technique in this method.
- patent literature 2 has disclosed a method of removing defects by densifying a shaped object by hot isostatic pressing.
- Patent literature 1 Japanese PCT National Publication No. 2007-521389 (International Publication WO2005/066380)
- Patent literature 2 Japanese Patent Laid-Open No. 2004-149826
- the present invention enables to provide a technique of solving the above problems.
- One aspect of the present invention provides a metal powder used for lamination-shaping which is an aluminum-based powder having a volume-based 50% particle diameter larger than or equal to 10 ⁇ m and smaller than 100 ⁇ m when a particle diameter distribution is measured by a laser diffraction-scattering method, a specific surface area smaller than or equal to 0.5 m 2 /g, and an oxygen amount larger than or equal to 3 mg/m 2 and less than or equal to 10 mg/m 2 per unit surface area,
- a relationship between a hydrogen amount (X ml in standard state) per 100 g of the aluminum-based powder and a specific surface area (Y m 2 /g), and a relationship between the hydrogen amount (X ml in standard state) and an oxygen amount (Z wt %), are respectively in accordance with following formulas: X/Y ⁇ 151 and, Z/X> 0.0022 preferably, X/Y ⁇ 130 and, Z/X ⁇ 0.003.
- Another aspect of the present invention provides a method of manufacturing a metal powder used for lamination-shaping, the method comprising:
- Still another aspect of the present invention provides a metal lamination-shaped object that is lamination-shaped by a three-dimensional lamination-shaping apparatus in a powder bed fusion type using the metal powder as mentioned above,
- a hydrogen amount is less than or equal to 3 ml per 100 g in standard state, and a relative density is more than or equal to 99%, in the metal lamination-shaped object.
- a subject of this example embodiment is to examine a defect generating mechanism in metal lamination-shaping using an aluminum-based powder, and control the amounts of hydrogen and oxygen per unit surface area contained in the powder, thereby obtaining a defect-free shaped object without any degassing step.
- Another subject of this example embodiment is to solve the problem that an aluminum-based powder absorbs moisture with time and the density of a lamination-shaped object decreases.
- this example embodiment solves the problem that when collecting and reusing a used powder after lamination-shaping, the powder absorbs moisture, so the initial shaped object density cannot be obtained.
- a method of obtaining an aluminum-based alloy powder of this example embodiment has the following two steps.
- An aluminum-based alloy powder is manufactured by gas atomization process, more preferably, centrifugal atomization process in an inert gas atmosphere in which the oxygen amount is controlled.
- the manufactured aluminum-based alloy powder is deaerated in an inert gas at 300° C. to 600° C. and more preferably 400° C. to 500° C., thereby obtaining an aluminum-based alloy powder of this example embodiment.
- An aluminum-based alloy powder to be used in this example embodiment is an Al—Si—Mg-based alloy.
- the alloy composition of the aluminum-based alloy powder is not limited to the Al—Si—Mg-based alloy, and it is possible to preferably use a wrought alloy (A1000 series, A2000 series, A3000 series, A4000 series, A5000 series, A6000 series, A7000 series, or A8000 series), a casting alloy, or a diecast alloy.
- a 900° C. molten metal of the obtained Al-10 wt % St-0.4 wt % Mg alloy is sprayed from a nozzle having a diameter of 2.2 mm, and atomized with 2.5-MPa high-pressure nitrogen.
- Atomized particles cooled in atmosphere are collected by a cyclone and bag filter.
- the atomized particles cooled in nitrogen adjusted to have an oxygen amount of 1 ppm or less are collected by the cyclone and bag filter.
- the atomization conditions and atomization atmosphere are that the atomization pressure was 2.0 to 5.0 MPa, and the atomization atmosphere was nitrogen, argon, or helium.
- alloy particles having a 50% particle size of 21 ⁇ m are further classified by a centrifugal force classifier, thereby removing most particles having a particle size of 7 ⁇ m or less. Then, particles obtained through a sieve having an opening of 45 ⁇ m (325 meshes) are evenly mixed by using a blender, thereby obtaining an Al-10 wt % Si-0.4 wt % Mg alloy powder of this example embodiment. Note that as this Al-10 wt % Si-0.4 wt % Mg alloy powder, it is also possible to use a powder obtained by collecting particles remaining on the sieve having an opening of 45 ⁇ m (325 meshes). That is, the 50% particle size is desirably 10 ⁇ m (inclusive) to 100 ⁇ m (exclusive).
- a 1,100° C. molten metal of the obtained Al-10 wt % Si-0.4 wt % Mg alloy is sprayed from a nozzle having a diameter of 1.7 mm onto a graphite rotary disk having a diameter of 100 mm and rotating at 20,000 rpm, which is installed in a nitrogen chamber having a diameter of 4 m and adjusted to have 0.01 wt % of oxygen, thereby obtaining aluminum-based particles.
- the distance between the spray nozzle and the rotary disk is 15 mm.
- the obtained aluminum-based particles are collected and further classified by the centrifugal force classifier, thereby removing most particles having a diameter of 7 ⁇ m or less.
- particles obtained through a sieve having an opening of 45 ⁇ m (325 meshes) are evenly mixed by using a blender, thereby obtaining an Al-10 wt % Si-0.4 wt % Mg alloy powder of this example embodiment.
- the obtained aluminum-based alloy powder is deaerated in an argon atmosphere as an inert gas at 300° to 600° C. and more preferably 400° C. to 500° C.
- the heating time is about 10 hours. Note that nitrogen or helium can also be used as the inert gas. Note also that the heating time need only be 1 to 100 hours.
- the aluminum-based alloy powder of this example embodiment manufactured by gas atomization process or centrifugal atomization process and deaerated in the inert gas atmosphere is used as a metal material for lamination-shaping, thereby shaping a metal lamination-shaped object by a three-dimensional lamination-shaping apparatus in a powder bed fusion type.
- the aluminum-based alloy powder and its lamination-shaped object were evaluated as follows.
- the powder of each example or each comparative example was dispersed for 180 sec by an ultrasonic wave, and the dispersion was placed in measurement-system circulating water and measured by using a laser refraction type diffraction particle diameter measurement apparatus (NIKKISO Microtrac MT-3300).
- the specific surface area was measured by the BET method (MOUNTECH Macsorb HM model-1210).
- the oxygen amount was measured by the inert gas melting-nondispersive infrared absorption method (HORIBA EMGA-920).
- Hydrogen amount of powder measured by the Ransley method.
- Hydrogen amount of lamination-shaped object measured by LECO JAPAN model RHEN602.
- a scanning electron microscope (JEOL JSM-6510A) was used to fix the powder of each example or each comparative example on a sample table without overlapping particles, and images enlarged by 500 times were electronically photographed in a plurality of fields. After that, at least 100 particles of the same sample were observed, and particles having satellites and particles having no satellites were counted.
- the fields were photographed such that the number of particles contained in one field was 15 or less.
- the field size was set such that the longitudinal and lateral sides were 4 to 12 times the 50% particle diameter.
- the overlapping of particles was minimized, and random extraction was performed, i.e., all vague particles such as apparently fused particles were counted as satellites.
- Roundness ⁇ c of each of 100 or more particles was measured by image analysis software (KEYENCE VHX-1000) in a plurality of fields photographed in the same manner as in item (3) above, thereby evaluating the average roundness.
- the Heywood diameter (an equivalent circle diameter) of each of 100 or more particles was calculated by the image analysis software (KEYENCE VHX-1000) in a plurality of fields photographed in the same manner as in item (3) above, and the number of particles smaller than 5 ⁇ m, the number of particles equal to or larger than 5 ⁇ m and smaller than 10 ⁇ m, and the number of particles equal to or larger than 10 ⁇ m were obtained.
- the abundance of the particles smaller than 5 ⁇ m was calculated by the following equation. If this abundance is 1.0 or less, the fluidity is high.
- a powder of each example or each comparative example thermally dissolved in a pressure vessel was measured by radio-frequency inductively coupled plasma-atomic emission spectroscopy (Thermo Fisher Scientific iCAP 6500 DUOView).
- a column having a diameter of 8 mm ⁇ a height of 15 mm was shaped, and the relative density with respect to the true density was measured by the Archimedes method.
- a column having a diameter of 6 mm ⁇ a length of 38 mm was shaped, and turned into a dumbbell shape having a parallel portion diameter of 3.5 mm and a parallel portion length of 18 mm. Then, a tensile test was conducted by using a universal tester (INSTRON M4206). The crosshead speed was set at 1 mm/min.
- a metal powder used for lamination-shaping of this example embodiment is an aluminum-based powder having a volume-based 50% particle diameter of 10 ⁇ m (inclusive) to 100 ⁇ m (exclusive) when the particle diameter distribution is measured by the laser diffraction-scattering method, a specific surface area of 0.5 m 2 /g or less, and an oxygen amount of 3 mg/m 2 (inclusive) to 10 mg/m 2 (inclusive) per unit surface area.
- the relationship between the hydrogen amount (X ml in standard state) per 100 g of the aluminum-based powder and the specific surface area (Y m 2 /g), and the relationship between the hydrogen amount (X ml in standard state) and the oxygen amount (Z wt %), are respectively in accordance with formulas: X/Y ⁇ 151 and Z/X> 0.0022, particularly, X/Y 130 and Z/X 0.003.
- a metal lamination-shaped object of this example embodiment shaped by a three-dimensional lamination-shaping apparatus in a powder bed fusion type using the above-mentioned metal powder has a hydrogen amount of 3 ml or less (in standard state) per 100 g, and a relative density of 99% or more.
- the metal powder obtained by the aluminum-based powder of this example embodiment achieves prominent effects as follows.
- Table 1 shows the manufacture of aluminum-based alloy powders of Examples 1 to 6 according to the present invention and Comparative Examples 1 to 6, lamination-shaped objects using the aluminum-based alloy powders, and the test results of the powders and objects.
- Example 2 Al—10%Si—0.4%Mg, 51.5 0.18 20.5 0.16 114 0.0078 8.9 ⁇ ⁇ 0.82 1.90 99.5 310 deaerated at 400° C.
- Example 3 Al—10%So—0.43%Mg, 22.1 0.24 27.7 0.21 115 0.0076 8.8 ⁇ ⁇ 0.82 2.78 99.2 305 deaerated at 425° C.
- Example 4 Al—10%Si—0.43%Mg, 28.1 0.17 16.7 0.06 98 0.0036 3.5 ⁇ ⁇ 0.93 1.78 99.7 320 centrifugal atomization process
- Example 5 Al—10%Si—0.43%Mg, 28.1 0.17 10.6 0.09 62 0.0085 5.3 ⁇ ⁇ 0.93 1.23 99.9 326 centrifugal atomization process, deaerated at 400° C.
- Example 6 Al—10%Si—0.4%Mg, 19.3 0.36 18.3 0.19 51 0.0104 5.3 X X 0.89 1.93 99.1 303 closed circuit, deaerated at 450° C.
- the obtained 900° C. molten metal was sprayed from a nozzle having a diameter of 2.2 mm, and atomized by 2.5-MPa high-pressure nitrogen. Atomized particles cooled in atmosphere were collected by a cyclone and bag filter. Of the atomized particles collected by the cyclone, alloy particles having a 50% particle diameter of 21 ⁇ m were further classified by a centrifugal force classifier, thereby removing most particles equal to or smaller than 7 ⁇ m.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- Example 2 A powder of Example 2 was obtained following the same procedures as in Example 1, except that a powder obtained by collecting particles remaining on the sieve having an opening of 45 ⁇ m was used, and the heating temperature in the argon atmosphere was set at 400° C.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- Example 3 A powder of Example 3 was obtained following the same procedures as in Example 1, except that the heating temperature in the argon atmosphere was set at 425° C.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- the obtained 1,100° C. molten metal was sprayed from a nozzle having a diameter of 1.7 mm onto a graphite rotary disk having a diameter of 100 mm and rotating at 20,000 rpm, which was installed in a nitrogen chamber having a diameter of 4 m and adjusted to have 0.01 wt % of oxygen, thereby obtaining aluminum-based particles.
- the distance between the spray nozzle and the rotary disk was 15 mm.
- the obtained aluminum-based particles were collected and further classified by the centrifugal force classifier, thereby removing most particles equal to or smaller than 7 ⁇ m. Then, particles obtained through a sieve having an opening of 45 ⁇ m (325 meshes) were evenly mixed by using a blender, thereby obtaining an Al-10 wt % Si-0.4 wt % Mg alloy powder of this example.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- Example 4 The aluminum-based powder obtained in Example 4 was heated in a 450° C. argon atmosphere for 10 hours.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- the obtained 900° C. molten metal was sprayed from a nozzle having a diameter of 2.2 mm, and atomized by 2.5-MPa high-pressure nitrogen. Atomized particles cooled in nitrogen adjusted to have an oxygen amount of 1 ppm or less were collected by the cyclone and bag filter.
- alloy particles having a 50% particle diameter of 21 ⁇ m were further classified by the centrifugal force classifier, thereby removing most particles equal to or smaller than 7 ⁇ m. Then, particles obtained through a sieve having an opening of 45 ⁇ m (325 meshes) were evenly mixed by using a blender, thereby obtaining an Al-10 wt % Si-0.4 wt % Mg alloy powder of this example. Furthermore, the obtained alloy powder was heated in an argon atmosphere at 450° C. for 10 hours.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- An aluminum-based powder of Comparative Example 1 was obtained following the same procedures as in Example 1, except that no heating process in an argon atmosphere was performed.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- An aluminum-based powder of Comparative Example 2 was obtained following the same procedures as in Example 2, except that no heating process in an argon atmosphere was performed.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- Table 1 shows the characteristic values of a commercially available, relatively fine aluminum-based powder for metal lamination-shaping, and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- Table 1 shows the characteristic values of a commercially available, relatively coarse aluminum-based powder for metal lamination-shaping, and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- An aluminum-based powder of Comparative Example 5 was obtained following the same procedures as in Example 6, except that no heating process in an argon atmosphere was performed.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- An aluminum-based powder of Comparative Example 6 was obtained following the same procedures as in Example 1, except that a deaeration process was performed in air at 400° C.
- Table 1 shows the characteristic values of this powder and the relative density and tensile strength of a lamination-shaped object manufactured by using the powder.
- Example 2 Al—10%Si—0.4%Mg, 20.5 0.16 99.5 22.3 0.17 99.4 21.2 0.16 99.5 deaerated at 400° C.
- Example 3 Al—10%Si—0.43%Mg, 27.7 0.21 99.2 28.4 0.21 99.2 28.0 0.21 99.2 deaerated at 425° C.
- Example 4 Al—10%Si—0.43%Mg, 16.7 0.06 99.7 17.1 0.07 99.7 16.9 0.07 99.7 centrifugal atomization process
- Example 5 Al—10%Si—0.43%Mg, 10.6 0.09 99.9 10.8 0.09 99.9 10.7 0.09 99.9 centrifugal atomization process, deaerated at 400° C.
- Example 6 Al—10%Si—0.4%Mg, 30.4 0.11 99.1 32.5 0.13 99.0 31.4 0.12 99.1 closed circuit, deaerated at 450° C. Comparative Al—10%Si—0.43%Mg 51.4 0.18 90.1 60.6 0.22 89.9 58.8 0.20 89.9 Example 1 Comparative Al—10%Si—0.4%Mg 40.4 0.18 93.3 47.3 0.20 92.5 45.2 0.19 92.8 Example 2 Comparative Commercially available 26.7 0.06 98.6 51.8 0.41 92.2 36.9 0.35 92.7 Example 3 Al—10%Si—0.4%Mg Comparative Commercially available 28.7 0.16 92.5 32.8 0.20 90.6 31.6 0.22 91.1 Example 4 Al—10%Si—0.4%Mg Comparative Al—10%Si—0.4%Mg Comparative Al—10%Si—0.4%Mg, 60.5 0.17 98.3 77.7 0.45 91.5 87.4 0.37 92.3 Example 5 closed circuit and not de
- Table 2 shows that the aluminum-based powders of the examples did not largely change the hydrogen amounts and oxygen amounts even after being stored in an open state, and the density of each lamination-shaped object did not decrease even after being aged, collected, and lamination-shaped again. In the comparative examples, however, the density of the lamination-shaped object manufactured from the powder having a Z/X value of less than 0.0022, particularly, less than 0.003 significantly decreased.
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Abstract
Description
X/Y<151 and,
Z/X>0.0022
preferably,
X/Y≤130 and,
Z/X≥0.003.
X/Y<151 and Z/X>0.0022, particularly, X/Y130 and Z/X0.003.
- (1) A defect-free robust metal lamination-shaped object which is difficult to manufacture by the conventional aluminum-based alloy powder is obtained.
- (2) The fluidity and spreadability which cannot be obtained by a well-known aluminum-based alloy powder are achieved. In the lamination-shaping step, therefore, a uniform powder bed is formed, and a dense shaped object is obtained.
- (3) The conventional aluminum-based powder has the problem that the oxygen amount and/or the hydrogen amount increases, and the density of the lamination-shaped object decreases. However, the metal powder used for lamination-shaping of this example embodiment is stable, and a high-density lamination-shaped object is obtained even when collecting and reusing the powder.
TABLE 1 |
Characteristics of Aluminum-Based Alloy Powders and Characteristics of 3D Lamination-shaped Objects using Powders |
Powder | Shaped | |||||||||||
hydro- | object | |||||||||||
Powder | gen | hydro- | ||||||||||
specific | amount | Powder | Oxygen | gen | Shaped | Shaped | ||||||
surface | X | oxygen | amount | amount | object | object |
Powder | area | [cc/ | amount | per unit | SEM image | [cc/ | relative | tensile | ||||
Composition of | D50 | Y | 100 g | Z | area | analysis results | 100 g | density | strength |
aluminum alloy | [μm] | [m2/g] | Al] | [%] | X/Y | Z/X | (mg/m2) | {circle around (1)} | {circle around (2)} | {circle around (3)} | Al] | (%) | [Mpa] | |
Example 1 | Al—10%Si—0.4%Mg, | 22.1 | 0.24 | 23.8 | 0.21 | 99 | 0.0088 | 8.8 | ◯ | ◯ | 0.82 | 2.04 | 99.7 | 316 |
deaerated at 450° C. | ||||||||||||||
Example 2 | Al—10%Si—0.4%Mg, | 51.5 | 0.18 | 20.5 | 0.16 | 114 | 0.0078 | 8.9 | ◯ | ◯ | 0.82 | 1.90 | 99.5 | 310 |
deaerated at 400° C. | ||||||||||||||
Example 3 | Al—10%So—0.43%Mg, | 22.1 | 0.24 | 27.7 | 0.21 | 115 | 0.0076 | 8.8 | ◯ | ◯ | 0.82 | 2.78 | 99.2 | 305 |
deaerated at 425° C. | ||||||||||||||
Example 4 | Al—10%Si—0.43%Mg, | 28.1 | 0.17 | 16.7 | 0.06 | 98 | 0.0036 | 3.5 | ◯ | ◯ | 0.93 | 1.78 | 99.7 | 320 |
centrifugal atomization | ||||||||||||||
process | ||||||||||||||
Example 5 | Al—10%Si—0.43%Mg, | 28.1 | 0.17 | 10.6 | 0.09 | 62 | 0.0085 | 5.3 | ◯ | ◯ | 0.93 | 1.23 | 99.9 | 326 |
centrifugal atomization | ||||||||||||||
process, deaerated at | ||||||||||||||
400° C. | ||||||||||||||
Example 6 | Al—10%Si—0.4%Mg, | 19.3 | 0.36 | 18.3 | 0.19 | 51 | 0.0104 | 5.3 | X | X | 0.89 | 1.93 | 99.1 | 303 |
closed circuit, deaerated | ||||||||||||||
at 450° C. | ||||||||||||||
Compar- | Al—10%Si—0.43%Mg | 22.1 | 0.24 | 51.4 | 0.18 | 214 | 0.0035 | 7.5 | ◯ | ◯ | 0.82 | 4.82 | 90.1 | 290 |
ative | ||||||||||||||
Example 1 | ||||||||||||||
Compar- | Al—10%Si—0.4%Mg | 51.5 | 0.18 | 40.4 | 0.18 | 224 | 0.0045 | 10.0 | ◯ | ◯ | 0.82 | 3.74 | 93.3 | 293 |
ative | ||||||||||||||
Example 2 | ||||||||||||||
Compar- | Commercially available | 29.0 | 0.24 | 26.7 | 0.06 | 111 | 0.0022 | 2.5 | X | X | 0.90 | 1.70 | 98.6 | 297 |
ative | Al—10%Si—0.4%Mg | |||||||||||||
Example 3 | ||||||||||||||
Compar- | Commercially available | 45.5 | 0.19 | 28.7 | 0.16 | 151 | 0.0056 | 8.4 | ◯ | ◯ | 0.68 | 3.00 | 92.5 | 280 |
ative | Al—10%Si—0.4%Mg | |||||||||||||
Example 4 | ||||||||||||||
Compar- | Al—10%Si—0.4%Mg, | 19.1 | 0.34 | 60.5 | 0.17 | 178 | 0.0028 | 5.0 | X | X | 0.88 | 4.11 | 98.3 | 285 |
ative | closed circuit and | |||||||||||||
Example 5 | not deaerated | |||||||||||||
Compar- | Al—10%Si—0.4%Mg, | 22.3 | 0.22 | 28.5 | 0.33 | 130 | 0.0116 | 15.0 | ◯ | ◯ | 0.83 | 2.1 | 93.5 | 275 |
ative | deaerated at 400° C. | |||||||||||||
Example 6 | in air | |||||||||||||
SEM image analysis results | ||||||||||||||
{circle around (1)} ◯: when the number of particles having diameters of 5 μm or less × 3 ≤ the number of particles having diameters of 10 μm or more, | ||||||||||||||
X: in other cases | ||||||||||||||
{circle around (2)} ◯: when the number of particles having satellites ≤ the number of particles having no satellites, | ||||||||||||||
X: in other cases | ||||||||||||||
{circle around (3)} Average roundness |
TABLE 2 |
Changes in Hydrogen Amounts and Oxygen Amounts of Aluminum Alloy Powders and Lamination-shaped Object Densities |
Immediately after manufacture (unsealing) |
Powder | Powder | Shaped object |
hydrogen | oxygen | relative | After storage at room | Collected after lamination- | ||
Aluminum alloy | amount | amount | density | temperature for 1 month | shaping (5 times) |
composition | [cc/100 gAl] | [%] | (%) | [cc/100 gAl] | [%] | (%) | (cc/100 gAl] | [%] | (%) | |
Example 1 | Al—10%Si—0.4%Mg, | 23.8 | 0.21 | 99.7 | 24.1 | 0.22 | 99.6 | 23.9 | 0.21 | 99.6 |
deaerated at 450° C. | ||||||||||
Example 2 | Al—10%Si—0.4%Mg, | 20.5 | 0.16 | 99.5 | 22.3 | 0.17 | 99.4 | 21.2 | 0.16 | 99.5 |
deaerated at 400° C. | ||||||||||
Example 3 | Al—10%Si—0.43%Mg, | 27.7 | 0.21 | 99.2 | 28.4 | 0.21 | 99.2 | 28.0 | 0.21 | 99.2 |
deaerated at 425° C. | ||||||||||
Example 4 | Al—10%Si—0.43%Mg, | 16.7 | 0.06 | 99.7 | 17.1 | 0.07 | 99.7 | 16.9 | 0.07 | 99.7 |
centrifugal atomization | ||||||||||
process | ||||||||||
Example 5 | Al—10%Si—0.43%Mg, | 10.6 | 0.09 | 99.9 | 10.8 | 0.09 | 99.9 | 10.7 | 0.09 | 99.9 |
centrifugal atomization | ||||||||||
process, deaerated at | ||||||||||
400° C. | ||||||||||
Example 6 | Al—10%Si—0.4%Mg, | 30.4 | 0.11 | 99.1 | 32.5 | 0.13 | 99.0 | 31.4 | 0.12 | 99.1 |
closed circuit, deaerated | ||||||||||
at 450° C. | ||||||||||
Comparative | Al—10%Si—0.43%Mg | 51.4 | 0.18 | 90.1 | 60.6 | 0.22 | 89.9 | 58.8 | 0.20 | 89.9 |
Example 1 | ||||||||||
Comparative | Al—10%Si—0.4%Mg | 40.4 | 0.18 | 93.3 | 47.3 | 0.20 | 92.5 | 45.2 | 0.19 | 92.8 |
Example 2 | ||||||||||
Comparative | Commercially available | 26.7 | 0.06 | 98.6 | 51.8 | 0.41 | 92.2 | 36.9 | 0.35 | 92.7 |
Example 3 | Al—10%Si—0.4%Mg | |||||||||
Comparative | Commercially available | 28.7 | 0.16 | 92.5 | 32.8 | 0.20 | 90.6 | 31.6 | 0.22 | 91.1 |
Example 4 | Al—10%Si—0.4%Mg | |||||||||
Comparative | Al—10%Si—0.4%Mg, | 60.5 | 0.17 | 98.3 | 77.7 | 0.45 | 91.5 | 87.4 | 0.37 | 92.3 |
Example 5 | closed circuit and | |||||||||
not deaerated | ||||||||||
Comparative | Al—10%Si—0.4%Mg, | 28.5 | 0.33 | 93.5 | 29.4 | 0.34 | 93.3 | 29.1 | 0.33 | 93.4 |
Example 6 | deaerated in air at | |||||||||
400° C. | ||||||||||
Aging Stability Test
Claims (10)
X/Y<151 and,
Z/X>0.0022.
X/Y≤130 and,
Z/X≥0.003.
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